Hydrochloric Acid → 1-(4-Fluorophenyl)-1, 4-dihydro-indeno [1, 2-c] pyrazole

HRID 366383

반응식

HRID 366383 반응식
O[CH:2]=[C:3]1[CH2:11][C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]1=O.Cl.[F:14][C:15]1[CH:20]=[CH:19][C:18]([NH:21][NH2:22])=[CH:17][CH:16]=1.Cl>C(O)C>[F:14][C:15]1[CH:20]=[CH:19][C:18]([N:21]2[C:4]3[C:5]4[C:10]([CH2:11][C:3]=3[CH:2]=[N:22]2)=[CH:9][CH:8]=[CH:7][CH:6]=4)=[CH:17][CH:16]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 699814-Fluorophenylhydrazine hydrochlorideHCID 37648821H-Inden-1-one, 2,3-dihydro-2-(hydroxymethylene)-

생성물 1

HCID 122910661-(4-Fluorophenyl)-1, 4-dihydro-indeno [1, 2-c] pyrazole

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2-Hydroxymethylene indan-1-one, (Example 1(ii) (a) (4.004 g; 250 mmol), p-fluorophenyl hydrazine hydrochloride (Aldrich) (4.106 g; 25.25 mmol) 10M hydrochloric acid (1 cm3) and ethanol (30 cm3), were heated under reflux for 19 hours. After cooling, the solvent was evaporated under reduced pressure, then taken up in dichloromethane and washed with 2M NaOH. The organic layer was separated, dried (Na2SO4), filtered and concentrated in vacuo. Purification by Kugelrohr distillation (140° C.; 0.01 mmHg) afforded a yellow solid, m.p. 104-105° C.

후처리

  1. temperatureunder reflux for 19 hours
  2. temperatureAfter cooling
  3. customthe solvent was evaporated under reduced pressure
  4. washwashed with 2M NaOH
  5. customThe organic layer was separated
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customPurification
  10. distillationby Kugelrohr distillation (140° C.; 0.01 mmHg)
  11. customafforded a yellow solid, m.p. 104-105° C.

출처 및 근거

ORD 기록
ord-538bde8ff3034153b72fd8cf2836b91c
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06130228

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